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Structural and magnetic properties of ZnNi xO thin films and diluted magnetic semiconductors have been investigated. This sample has been synthesized using a spray pyrolysis technique with a stoechiometric mixture of zinc acetate (C4H6O4Zn2H2O) and Nickel acetate (C4H6O4Ni 2H2O) on a heated glass substrate at 450C. The films were characterized by X-ray diffraction (XRD), UV-Vis spectrophotometry and Hall Effect measurements. These films of ZnO crystallized in the hexagonal Wurtzite structure. The optical study showed that the band-gap energy was increased, from 3.3eV to 3.5eV, with increasing the Ni concentration. The film resistivity was affected by Ni-doping, and the best resistivity value 1.1510 ( cm) was obtained for the film doped with 2 at.% Ni. The electronic structure and optical properties of the Wurtzite structure ZnNi xO were obtained by first-principles calculations using the Korringa-Kohn-Rostoker method combined with the coherent potential approximation (CPA), as well as CPA confirm our results. [ABSTRACT FROM AUTHOR]